CN102393427B - Analyzing method of Ni content in melted steel ingot - Google Patents
Analyzing method of Ni content in melted steel ingot Download PDFInfo
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- CN102393427B CN102393427B CN 201110341433 CN201110341433A CN102393427B CN 102393427 B CN102393427 B CN 102393427B CN 201110341433 CN201110341433 CN 201110341433 CN 201110341433 A CN201110341433 A CN 201110341433A CN 102393427 B CN102393427 B CN 102393427B
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Abstract
An analyzing method of Ni content in a melted steel ingot belongs to the test method of laboratories in metallurgy industries, and comprises the following operation links: weighing samples, dissolving samples, filtering, cleaning, ashing, melting and cooling filter matters, combining filtrate, adjusting the degree of acidity of the solution, settling, aging, filtering, drying and calculating. The analyzing method effectively overcomes the defects that undissolved substances often can not be resolved thoroughly in the analyzing process of melting the steel ingot by stainless steel slag or dust removing ash, so that the sample can be resolved thoroughly, and further the effects of accurate and reliable test result can be achieved.
Description
Technical field:
The invention belongs to smelter laboratory assay method, be specifically related to a kind of chemico-analytic method of Ni content in melted steel ingot.
Background technology
The melted steel ingot that stainless steel slag or dedusting ash remelting form is a kind of slag regenerant between the pig iron and stainless steel, as steel scrap supply steel mill, needs to analyze C, S, P, Cr, Ni, TFe content.The processing factory laboratory is to use iron and steel methods analyst Ni content wherein at present, and there is following defective in this method: have the part insolubles in the sample course of dissolution and occur, sample is difficult to dissolve fully, will have a strong impact on precision of analysis.
Summary of the invention:
The present invention proposes the analytical approach of Ni content in a kind of melted steel ingot, its objective is the defective in overcoming above-mentioned Ni ultimate analysis process, and a kind of thoroughly method of dissolved samples is provided, thereby makes analysis result accurately, reliably.
Technical scheme of the present invention comprises and takes sample---dissolved samples---filter, clean---filtrate ashing, melting, cooling---filtrate mergings---adjust solution acidity---operation link of calculating---is filtered, dries---in precipitation, ageing, and concrete steps are:
(1), stainless steel is claimed sample 0.500g is placed in the beaker of 600ml;
(2), add chloroazotic acid 20ml in the beaker, the beaker cover surface plate is placed on electric hot plate, with the low temperature shelves heating of electric hot plate, produce a large amount of minute bubbles, until minute bubbles disappear, then drip hydrofluorite 3-4 in the beaker and drip, then add perchloric acid 5ml, make that in beaker, solution is syrupy shape;
(3), add in the beaker hydrochloric acid 10ml to make solubility salt dissolving in beaker, then add water the total solution in beaker be controlled in 100ml, use fast quantification filter paper to be filtered into former filtrate to the solution in beaker;
(4), filter paper and the particle that is adsorbed on filter paper are placed in platinum crucible, particle charing on platinum crucible is placed in and makes filter paper on electric furnace and be adsorbed on filter paper becomes carbide, the platinum crucible that carbide will be housed is again put into calcination on muffle furnace, calcination temperature is 1000 ℃, calcination 20 minutes becomes calcination with the carbide ashing;
(5), platinum crucible taken out naturally cool to room temperature,---dripping two 1+1 sulfuric acid solutions---adds the hydrofluorite of 5ml then to drip the wetting calcination of 2ml distilled water successively in platinum crucible; Platinum crucible is placed in electric hot plate, and electric plate temperature is 70-100 ℃, evaporates the liquid in platinum crucible, and the sulfuric acid cigarette to platinum crucible emits to the greatest extent; And then platinum crucible was put into the muffle furnace calcination 10-15 minute, calcination temperature is 1000 ℃; Take out platinum crucible and make platinum crucible naturally cool to room temperature; Add potassium pyrosulfate 4 grams in platinum crucible, with platinum crucible
PutIn muffle furnace, muffle furnace is set as 700-800 ℃, and platinum crucible melts to aglow bright;
(6), take off the naturally cooling rear generation potassium pyrosulfate frit of platinum crucible; The potassium pyrosulfate frit is placed in former filtrate makes the molten dissolving fully of potassium pyrosulfate, clean platinum crucible with distilled water, in former filtrate beaker, total solution is controlled between 350-400ml;
(7), add successively hydrochloric acid 10ml in former filtrate beaker---citric acid 10ml; Then add while stirring ammoniacal liquor to transfer the solution pH value, making the solution pH value is 8-9, with the check of PH test paper;
(8), add boiling water in former filtrate beaker, making the volume in former filtrate beaker is 480ml, and in former filtrate beaker, solution temperature is controlled at more than 75 ℃, slowly adds dimethylglyoxime solution 50ml in solution, stir while adding, generate red dimethylglyoxime nickel precipitation;
(9), former filtrate beaker is placed in ageing on electric hot plate, be incubated 45 minutes, temperature is controlled at 70 ℃;
(10), use sintered filter funnel to filter dimethylglyoxime nickel precipitation, the weak aqua ammonia washing dimethylglyoxime nickel precipitation with 2% 5-8 time, then wash 3-5 time with distilling is got rid of the water column of funnel bottom;
(11), dimethylglyoxime nickel precipitation is put into baking oven together with funnel, oven temperature is set as 135 ℃, dry 2 hours, takes out the exsiccator of putting into of funnel after drying and precipitation, naturally cools to room temperature, the weight of steelyard slepsydra bucket and precipitation.
(12), calculate Ni content in melted steel ingot
In formula: the sedimentary quality of G_____ is to be deducted the Mass Calculation of sky funnel by the quality with sedimentary funnel, and unit is g;
0.2032_____ the conversion coefficient of dimethylglyoxime nickel and nickel;
0.5000_____ the sample weighting amount of analytical sample, unit are g.
Note:
(1) sintered filter funnel: should clean up before 1. using, put into baking oven, oven temperature is set as 135 ℃ of left and right, dries 1 hour, takes out and is placed in exsiccator, is cooled to room temperature, weighs rear standby.Do water column when 2. using and be convenient to fast filtering.3. rinse in clear water after using and put into beaker, add 2% watery hydrochloric acid and be placed in foam washing on electric furnace, to be cleanedly clean standby with distilled water again after clean.
(2) empty funnel is placed in exsiccator with sedimentary funnel oven dry is arranged, and the type of cooling should be consistent with cool time.
(3) described solubility salt produces in step 2, is after " in beaker, solution is syrupy shape ", separates out because the minimizing of solution amount has some solubility salts.
The present invention has effectively overcome the defective that in stainless steel slag or dedusting ash melted steel ingot analytic process, the frequent insolubles that occurs can not thoroughly decompose, and sample can thoroughly be dissolved, thereby reaches accurate, the reliable effect of result of laboratory test.
Embodiment:
Embodiment:The present embodiment is that in May, 2007 is in the chemical examination example of Shanxi Stainless-steel Jiont Stock Company of Taiyuan Iron﹠Steel Complex processing factory.
Practice shows, result of use of the present invention is good, easily for operating personnel grasp, realized that sample thoroughly decomposes, and has guaranteed precision of analysis.
Embodiment:
Dedusting ash melted steel ingot sample sample weighting amount is 0.500g, and sample is placed in the beaker in 600ml.
Add chloroazotic acid 20ml in beaker, the beaker cover surface plate is placed on electric hot plate, and the low temperature shelves heating with electric hot plate produces a large amount of minute bubbles, until minute bubbles disappear, carries out the sample dissolving; Drip hydrofluorite 3-4 in the beaker and drip, continue the low temperature shelves with electric hot plate, until reaction stops, adding perchloric acid 5ml, continue the liquid that the low temperature shelves with electric hot plate are heated in beaker and be syrupy shape.
Add hydrochloric acid 10ml in beaker, the solubility salt in beaker is dissolved fully; Then add water, the solution in beaker is controlled in 100ml; Use fast quantification filter paper that the solution in beaker is filtered; After the distilled water flushing beaker 7-8 of 70-80 ℃ time, the aqueous solution of cleaning and filtered fluid combine and are referred to as former filtrate, and the beaker that holds former filtrate is referred to as former filtrate beaker.
Filter paper and the particle that is adsorbed on filter paper are placed in platinum crucible, are placed in charing on electric furnace, then put into 1000 ℃ of muffle furnace set temperatures, calcination 20 minutes is with filter paper and be adsorbed on particle ashing on filter paper.
After ashing, platinum crucible is taken out and naturally cool to room temperature, add successively two hydrofluorite that drip, drip two 1+1 sulfuric acid solutions, 5ml in the platinum crucible; Platinum crucible is placed on electric hot plate, with the solution in electric hot plate low temperature gear evaporation platinum crucible, treats to emit the sulfuric acid cigarette in platinum crucible until the sulfuric acid cigarette is emitted to the greatest extent; And then platinum crucible is put into muffle furnace, 1000 ℃ of muffle furnace set temperatures, calcination 10-15 minute.
Take out platinum crucible and naturally cool to room temperature, add potassium pyrosulfate 4 grams in platinum crucible, then platinum crucible is placed in muffle furnace melts to aglow brightly, muffle furnace is set as between 700-800 ℃.
Take off platinum crucible naturally cooling after, the potassium pyrosulfate frit is placed in former filtrate beaker, make that potassium pyrosulfate is molten to be dissolved in former filtrate fully; Use distilled water that platinum crucible is cleaned, the water of washing platinum crucible adds in former filtrate beaker, and in former filtrate beaker, solution is controlled between 350-400ml.
Add hydrochloric acid 10ml in former filtrate beaker, then adding citric acid 10ml; Then add while stirring ammoniacal liquor to transfer the solution pH value, making the solution pH value is that 8-9(can not be greater than 10), with the check of PH test paper;
Add boiling water in the former filtrate beaker and make the volume of solution in the filtrate beaker reach 480ml, in former filtrate beaker, solution temperature is controlled at more than 75 ℃;
Slowly add dimethylglyoxime solution 50ml in solution, stir while adding, generating red complex is dimethylglyoxime nickel precipitation.
Former filtrate beaker is placed in ageing on electric hot plate, is incubated 45 minutes, temperature is controlled at 70 ℃.
Use sintered filter funnel to filter dimethylglyoxime nickel precipitation, the weak aqua ammonia washing dimethylglyoxime nickel precipitation with 2% 5-8 time, then with distillation washing 3-5 time, get rid of the water column of funnel bottom.
Dimethylglyoxime nickel precipitation is put into baking oven together with funnel, and oven temperature is set as 135 ℃ of left and right, dry 2 hours, takes out the exsiccator of putting into of funnel after drying and precipitation, naturally cools to room temperature, the weight of steelyard slepsydra bucket and precipitation.
Calculate nickel content according to computing formula.
Computing formula:
In formula: the sedimentary quality of G_____ is to be deducted the Mass Calculation of sky funnel by the quality with sedimentary funnel, and unit is g.
0.2032_____ the conversion coefficient of dimethylglyoxime nickel and nickel.
0.5000_____ the sample weighting amount of analytical sample, unit are g.
G1=34.0351?g?-33.9234?g?=0.1117?g
G2=35.7775?g?-35.6646?g?=0.1129?g
Data are as follows:
Described ashing is about to the process that the charcoal in filter paper burnouts.
Described ageing namely by with solution insulation, standing, impels dimethylglyoxime and nickel element to form stable bulky grain precipitation and the more pure process of precipitation.
Claims (1)
1. the analytical approach of Ni content in a melted steel ingot
,It is characterized in that comprising following step successively:
(1), stainless steel is claimed sample 0.500g is placed in the beaker of 600ml;
(2), add chloroazotic acid 20ml in the beaker, the beaker cover surface plate is placed on electric hot plate, with the low temperature shelves heating of electric hot plate, produce a large amount of minute bubbles, until minute bubbles disappear, then drip hydrofluorite 3-4 in the beaker and drip, then add perchloric acid 5ml, make that in beaker, solution is syrupy shape;
(3), add in the beaker hydrochloric acid 10ml to make solubility salt dissolving in beaker, then add water the total solution in beaker be controlled in 100ml, use fast quantification filter paper that the solution in beaker is filtered; After the distilled water flushing beaker 7-8 of 70-80 ℃ time, the aqueous solution of cleaning and filtered fluid combine and are referred to as former filtrate, and the beaker that holds former filtrate is referred to as former filtrate beaker;
(4), filter paper and the particle that is adsorbed on filter paper are placed in platinum crucible, particle charing on platinum crucible is placed in and makes filter paper on electric furnace and be adsorbed on filter paper becomes carbide, the platinum crucible that carbide will be housed is again put into calcination on muffle furnace, calcination temperature is 1000 ℃, calcination 20 minutes becomes calcination with the carbide ashing;
(5), platinum crucible taken out naturally cool to room temperature,---dripping two 1+1 sulfuric acid solutions---adds the hydrofluorite of 5ml then to drip the wetting calcination of 2ml distilled water successively in platinum crucible; Platinum crucible is placed in electric hot plate, and electric plate temperature is 70-100 ℃, evaporates the liquid in platinum crucible, and the sulfuric acid cigarette to platinum crucible emits to the greatest extent; And then platinum crucible was put into the muffle furnace calcination 10-15 minute, calcination temperature is 1000 ℃; Take out platinum crucible and make platinum crucible naturally cool to room temperature; Add potassium pyrosulfate 4 grams in platinum crucible, with platinum crucible
PutIn muffle furnace, muffle furnace is set as 700-800 ℃, and platinum crucible melts to aglow bright;
(6), take off the naturally cooling rear generation potassium pyrosulfate frit of platinum crucible; The potassium pyrosulfate frit is placed in former filtrate beaker, potassium pyrosulfate is melted be dissolved in fully in former filtrate; Use distilled water that platinum crucible is cleaned, the water of washing platinum crucible adds in former filtrate beaker, and in former filtrate beaker, solution is controlled between 350-400ml;
(7), add successively hydrochloric acid 10ml in former filtrate beaker---citric acid 10ml; Then add while stirring ammoniacal liquor to transfer the solution pH value, making the solution pH value is 8-9, with the check of PH test paper;
(8), add boiling water in former filtrate beaker, making the volume in former filtrate beaker is 480ml, and in former filtrate beaker, solution temperature is controlled at more than 75 ℃, slowly adds dimethylglyoxime solution 50ml in solution, stir while adding, generate red dimethylglyoxime nickel precipitation;
(9), former filtrate beaker is placed in ageing on electric hot plate, be incubated 45 minutes, temperature is controlled at 70 ℃;
(10), use sintered filter funnel to filter dimethylglyoxime nickel precipitation, the weak aqua ammonia washing dimethylglyoxime nickel precipitation with 2% 5-8 time, then wash 3-5 time with distilling is got rid of the water column of funnel bottom;
(11), dimethylglyoxime nickel precipitation is put into baking oven together with funnel, oven temperature is set as 135 ℃, dry 2 hours, takes out the exsiccator of putting into of funnel after drying and precipitation, naturally cools to room temperature, the weight of steelyard slepsydra bucket and precipitation;
(12), calculate Ni content in melted steel ingot
In formula: the sedimentary quality of G_____ is to be deducted the Mass Calculation of sky funnel by the quality with sedimentary funnel, and unit is g;
0.2032_____ the conversion coefficient of dimethylglyoxime nickel and nickel;
0.5000_____ the sample weighting amount of analytical sample, unit are g.
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| CN109211812A (en) * | 2018-10-21 | 2019-01-15 | 福建通海镍业科技有限公司 | The analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy |
| CN109283023B (en) * | 2018-11-06 | 2024-04-16 | 华北电力大学（保定） | Experimental device for simulating influence of smoke content on sulfur trioxide concentration and application method |
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